Determination of total amount of rare earth elements and its component in iron concentrate by inductively coupled plasma mass spectrometry with microwave digestion
YAO Mingxing1,2,3, GUO Xiaorui1,2,3, MAO Xiangju1,2,3, WANG Tiantian1,2,3, NI Wenshan*1,2,3
1. Zhengzhou Institute of Multipurpose Utilization of Mineral Resources,CAGS,Zhengzhou 450006,China; 2. China National Engineering Research Center for Utilization of Industrial Minerals,Zhengzhou 450006,China; 3. Key Laboratory for Polymetallic Ores′ Evaluation and Utilization,MNR,Zhengzhou 450006,China
Abstract：The accurate determination of total amount of rare earth elements and its component in iron concentrate is of great significance for the comprehensive utilization of iron concentrate. In this study, the iron concentrate sample was dissolved by microwave digestion with 6 mol/L HCl. Iron (Ⅲ) in matrix was extracted with methyl isobutyl ketone to overcome the matrix effect. The internal standard correction was conducted with 50 ng/mL Re. The total amount of rare earth elements and its component in solution were determined by inductively coupled plasma mass spectrometry (ICP-MS) using standard mode. The determination of total amount of rare earth elements and its component in iron concentrate was realized. The influence of matrix effect on the determination was investigated. The results showed that the recoveries of rare earth elements were between 6% and 31% if the sample was directly determined by ICP-MS after microwave digestion, implying that the influence of matrix effect on the determination could not be ignored. After microwave digestion, the iron matrix was removed by methyl isobutyl ketone extraction. Then the solution was determined by ICP-MS, and the recoveries of rare earth elements were between 96% and 103%. Therefore, before determination, the methyl isobutyl ketone extraction was adopted after digesting the sample to separate the iron matrix from testing elements. Under the optimal experimental conditions, the mass concentration of rare earth elements in range of 5-100 ng/mL showed a good linear relationship with the corresponding MS signal intensity. The correlation coefficients (r) of calibration curves were between 0.999 2 and 0.999 9. The limits of detection of method were between 0.000 1 ng/mL and 0.060 5 ng/mL. The proposed method was applied for the determination of total amount of rare earth elements and its component in iron concentrate. The relative standard deviations (RSD, n=6) of determination results were between 2.3% and 4.2%. The spiked recoveries of total amount of rare earth elements and its component were between 92% and 108%, which could meet the analysis requirements on spiked recovery in national geological and mineral industry standard DZ/T 0130-2006.
姚明星, 郭晓瑞, 毛香菊, 王甜甜, 倪文山. 微波消解-电感耦合等离子体质谱法测定铁精矿中稀土元素分量和总量[J]. 冶金分析, 2024, 44(2): 10-17.
YAO Mingxing, GUO Xiaorui, MAO Xiangju, WANG Tiantian, NI Wenshan. Determination of total amount of rare earth elements and its component in iron concentrate by inductively coupled plasma mass spectrometry with microwave digestion. , 2024, 44(2): 10-17.
[1] 倪文山,刘长淼,姚明星,等.电感耦合等离子体质谱法测定磷灰石中稀土元素分量和总量[J].冶金分析,2016,36(7):69-73. NI Wenshan,LIU Changmiao,YAO Mingxing,et al.Determination of the total amount of rare earth elements and its component in apatite by inductively coupled plasma mass spectrometry[J].Metallurgical Analysis,2016,36(7):69-73. [2] 岩石矿物分析编写组.岩石矿物分析:第1分册[M].3版.北京:地质出版社,1991:675. [3] 贺谊.流动注射光度法测定江西两种稀土矿中的稀土总量[J].南昌大学学报(理科版),1999,23(1):90-94. HE Yi.Determination of total rare earth in two kinds of rare earth ores of absorbed form in Jiangxi by flow injection-spectrophotometry[J].Journal of Nanchang University(Natural Science),1999,23(1):90-94. [4] 夏峰林,孔雪艳,史秀梅.分光光度法测定高放废液中的稀土总量[J].核化学与放射化学,2020,42(5):371-377. XIA Fenglin,KONG Xueyan,SHI Xiumei.Determination of total rare earth in HLLW by spectrophotometry[J].Journal of Nuclear and Radiochemistry,2020,42(5):371-377. [5] 姜桂兰,曹淑琴,王多禧,等.化学-X-射线荧光光谱法测定地质样品中痕量稀土元素[J].分析化学,1994,22(1):47-50. JIANG Guilan,CAO Shuqin,WANG Duoxi,et al.Determination of rare earth elements in geological specimen by chemistry-X-ray fluorence spectrometry[J].Chinese Journal of Analytical Chemistry,1994,22(1):47-50. [6] 李小莉,张勤.粉末压片-X射线荧光光谱法测定土壤、水系沉积物和岩石样品中15种稀土元素[J].冶金分析,2013,33(7):35-40. LI Xiaoli,ZHANG Qin.Determination of fifteen rare earth elements in soil,stream sediment and rock samples by X-ray fluorescence spectrometry with pressed powder pellet[J].Metallurgical Analysis,2013,33(7):35-40. [7] 徐静,李宗安,李明来,等.微波消解-电感耦合等离子体原子发射光谱法测定稀土合金渣中主要稀土氧化物[J].冶金分析,2012,32(11):46-50. XU Jing,LI Zongan,LI Minglai,et al.Determination of main rare earth oxides in rare earth alloy slag by microwave digestion-inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2012,32(11):46-50. [8] 赵振.三种检测方法测定15种稀土元素总量比对分析[J].福建分析测试,2020,29(6):46-50. ZHAO Zhen.Comparative analysis of three detection methods determination total amount of 15 rare earth elements[J].Fujian Analysis and Testing,2020,29(6):46-50. [9] 许涛,崔爱端,杜梅,等.电感耦合等离子体发射光谱法测定稀土铌钽矿中稀土元素和钍量[J].岩矿测试,2009,28(6):549-552. XU Tao,CUI Aiduan,DU Mei,et al.Determination of rare earth elements and thorium in RE-Nb-Ta ores by inductively coupled plasma-atomic emission spectrometry[J].Rock and Mineral Analysis,2009,28(6):549-552. [10] 周国兴,刘玺祥,崔德松.碱熔ICP-MS法测定岩石样品中稀土等28种金属元素[J].质谱学报,2010,31(2):120-124. ZHOU Guoxing,LIU Xixiang,CUI Desong.Determination of 28 elements including rare earth elements by ICP-MS in alkali melted rock sample[J].Journal of Chinese Mass Spectrometry,2010,31(2):120-124. [11] HU Shenghong,HU Zhaochu,LIU Yongsheng,et al.Determination of sub-trace Sc,Y and Ln in carbonate by ICP-MS with inter-element matrix-matched technique[J].Journal of Rare Earths,2003,21(2):124-128. [12] 曹心德,王晓蓉,尹明,等.微波消解-电感耦合等离子体质谱法测定土壤中微量稀土元素[J].分析化学,1999,27(6):679-683. CAO Xinde,WANG Xiaorong,YIN Ming,et al.Determination of trace rare earth elements in soils by inductively coupled plasma-mass spectrometry after microwave digestion for sample preparation[J].Chinese Journal of Analytical Chemistry,1999,27(6):679-683. [13] 施意华,邱丽,唐碧玉,等.电感耦合等离子体质谱法测定离子型稀土矿中离子相稀土总量及分量[J].冶金分析,2014,34(9):14-19. SHI Yihua,QIU Li,TANG Biyu,et al.Determination of total ionic-phase rare earth and component in ion-adsorption rare earth ore by inductively coupled plasma mass spectrometry[J].Metallurgical Analysis,2014,34(9):14-19. [14] 张立锋,张秀艳,张翼明,等.电感耦合等离子体质谱法测定镧镁合金中稀土杂质[J].冶金分析,2014,34(6):33-37. ZHANG Lifeng,ZHANG Xiuyan,ZHANG Yiming,et al.Determination of rare earth impurities in lanthanum-magnesium alloy by inductively coupled plasma mass spectrometry[J].Metallurgical Analysis,2014,34(6):33-37. [15] 刘虎生,邵宏翔.电感耦合等离子体质谱技术与应用[M].北京:化学工业出版社,2005:120-121. [16] 王小如.电感耦合等离子体质谱应用实例[M].北京:化学工业出版社,2005:271. [17] 张宏丽,高小飞,姚明星,等.微波消解-电感耦合等离子体质谱法测定赤泥中稀土总量及分量[J].稀土,2019,40(3):96-101. ZHANG Hongli,GAO Xiaofei,YAO Mingxing,et al.Microwave dissolving-inductively coupled plasma mass spectrometric determination of total and individual REE in red mud[J].Chinese Rare Earths,2019,40(3):96-101. [18] 施先义,廖静婷,王世彬.铝片还原-重铬酸钾滴定法测定硫铁矿中铁的改进[J].岩矿测试,2009,28(2):197-198. SHI Xianyi,LIAO Jingting,WANG Shibin.Improvement on the method for determination of iron in pyrites by potassium dichchromate titrimetry with aluminium tablet reduction[J].Rock and Mineral Analysis,2009,28(2):197-198. [19] 于汀汀,王蕾,郭琳,等.酸溶-电感耦合等离子体发射光谱测定不同类型铍矿中的主次量元素方法优化[J].岩矿测试,2023,42(5):923-933. YU Tingting,WANG Lei,GUO Lin,et al.Determination of 9 major and minor elements in beryllium ore by ICP-OES with acid dissolution[J].Rock and Mineral Analysis,2023,42(5):923-933.
